CN110635068B - Method for continuously printing OLED flexible display panel in roll-to-roll mode - Google Patents
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- H10K50/00—Organic light-emitting devices
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- H10K71/12—Deposition of organic active material using liquid deposition, e.g. spin coating
- H10K71/13—Deposition of organic active material using liquid deposition, e.g. spin coating using printing techniques, e.g. ink-jet printing or screen printing
- H10K71/135—Deposition of organic active material using liquid deposition, e.g. spin coating using printing techniques, e.g. ink-jet printing or screen printing using ink-jet printing
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Abstract
The invention provides a method for continuously printing an OLED flexible display panel in a roll-to-roll mode, which comprises the steps of blade-coating an anode coating liquid containing graphene on the surface of a polyimide film in a roll-to-roll continuous printing device, then carrying out ink-jet printing on a hole transport material and a hole injection layer material which are distributed at intervals on the surface of an anode, then carrying out ink-jet printing on a luminescent material, then carrying out ink-jet printing on an electron transport material and an electron injection layer material which are distributed at intervals, further pressing the electron transport material and the electron injection layer material with a film deposited with an alloy to form a cathode, and finally carrying out. The preparation method provided by the invention overcomes the defects of uneven printing, easy coffee effect formation and untight combination in direct ink-jet printing, improves the transmission efficiency, realizes controllable thickness and controllable precision, and is suitable for large-area, large-scale, continuous and stable preparation of the OLED flexible display panel.
Description
Technical Field
The invention relates to the technical field of preparation of OLED flexible display panels, in particular to a method for continuously printing OLED flexible display panels in a roll-to-roll mode.
Background
The OLED is an organic light emitting diode, and is an organic electroluminescent device having a self-luminous property. The LED is characterized in that organic micromolecules or polymeric materials are used as semiconductors in the LED. The structure of the main body OLED comprises: a Hole Transport Layer (HTL), an Emission Layer (EL), and an Electron Transport Layer (ETL). When power is supplied to a proper voltage, positive holes and negative charges are combined in the light-emitting layer to generate light, and red, green and blue RGB three primary colors are generated according to different formulas to form basic colors. The OLED is characterized by self-illumination, unlike the TFT LCD which requires backlight, and thus has high visibility and brightness, and secondly has low voltage requirement and high power saving efficiency, and is fast in response, light in weight, thin in thickness, simple in structure, low in cost, etc., and is considered as one of the most promising products in the 21 st century.
With the continuous development of display technologies, flexible OLED displays have the advantages of light weight, thinness, durability, and being capable of being rolled up, and become the next generation of display technologies with the most potential development. The development of flexible display technology has put new demands on the existing molding technology. The original technology of layer-by-layer deposition on a glass substrate cannot adapt to the development of flexible display.
The most important technical control in the production of OLEDs is how the organic layers are applied layer by layer to the substrate. The main technical processes at present are as follows: one is vacuum deposition or vacuum thermal evaporation, organic molecules in a vacuum chamber are slightly heated (evaporated), and then the molecules are condensed on a substrate with a lower temperature in the form of a thin film. This method is very costly, but inefficient; and the other is organic vapor deposition, in a low-pressure hot-wall reaction cavity, the carrier gas conveys evaporated organic molecules to a low-temperature base layer, and then the organic molecules are condensed into a film. The use of carrier gas can improve efficiency and reduce cost of OLEDs, but the process is complex and has low degrees of continuity.
Inkjet printing is a new technology for making flexible OLED displays in recent years. The OLED core material can be sprayed onto the base layer by using the ink-jet technology, like ink is sprayed onto paper during printing, the production cost of the OLED is greatly reduced, and the OLED can be printed onto a film with a very large surface area. However, in the specific inkjet printing, it is difficult to control the uniformity and robustness of printing in the specific industrial production due to the change of the electronic ink material and the change of the printing substrate.
Chinese invention patent application No. 201710986812.1 discloses a method for preparing a printed OLED display screen, which comprises the following steps: preparing a hole injection layer, a hole transport layer or an electron blocking layer on the anode substrate; forming a soluble fluorine-containing insulating layer by using a printing method to seal the whole substrate; printing a fluorine solvent on the soluble fluorine-containing insulating layer in an ink-jet mode, and washing all the sub-pixel pits; ink-jet printing droplets of a light-emitting material solution so that red, green and blue light-emitting layers are formed in the sub-pixel pits; preparing an electron injection layer, an electron transport layer or a hole blocking layer; and preparing a cathode by using a printing method or an evaporation method, and finally encapsulating to finish the preparation of the single printed OLED display screen. Chinese invention patent application No. 201710651649.3 discloses a method for preparing a printed OLED device, which comprises the following steps: (1) providing a substrate, wherein a pixel defining layer is arranged on the substrate and is provided with pixel pits corresponding to pixels; (2) depositing organic functional black water in the pixel pits by adopting a printing process, and drying to obtain an organic functional film layer; (3) placing the substrate with the organic functional film layer in an electric field for baking; (4) repeating the steps (2) and (3) to manufacture and form a plurality of organic functional film layers; (5) and manufacturing and packaging the top electrode according to a conventional method to obtain the printed OLED device.
In order to overcome the problems of uneven printing, easy coffee effect formation and untight combination existing in the direct ink-jet printing, a new ink-jet printing method is needed to be provided, and further, the large-scale continuous and stable preparation of the OLED flexible display panel is realized.
Disclosure of Invention
Aiming at the defects of uneven printing, easy coffee effect formation and untight combination in the current ink-jet printing process, which influence the large-scale preparation of the OLED flexible display panel, the invention provides a method for continuously printing an OLED flexible display panel in a roll-to-roll mode, which can overcome the defects, improve the transmission efficiency, realize the controllable thickness and the controllable precision and is suitable for preparing large-area OLED flexible display devices.
In order to solve the problems, the invention adopts the following technical scheme:
the invention provides a method for continuously printing an OLED flexible display panel in a roll-to-roll mode, which comprises the following specific processes:
(1) feeding the coiled polyimide film into a roll-to-roll continuous printing device, firstly carrying out blade coating to enable the anode coating liquid to be blade-coated on the surface of the polyimide film, and then carrying out pre-drying treatment;
(2) through non-contact ink-jet printing, alternately printing the ink of the hole injection layer material and the ink of the hole transport layer material on the surface of the anode at one time, and drying to form a hole transport layer; wherein the mass fraction of the silicon dioxide aerogel in the ink is 0.5-1%;
(3) printing red, green and blue luminescent material inks on the surface of the hole transport layer according to high pixel settings through non-contact ink-jet printing, and drying;
(4) alternately printing the ink of the electron injection layer and the ink of the electron transmission material on the surface of the anode at one time, and drying to form an electron transmission layer;
(5) and pressing the film deposited with the alloy on the electron transmission layer to form a cathode, and performing roller heat setting, packaging and coiling to obtain the OLED flexible display panel.
Preferably, the anode coating liquid is prepared by ultrasonically dispersing graphene in polytetrafluoroethylene emulsion, wherein the mass fraction of the graphene in the emulsion is 2-4%, and the solid content of the polytetrafluoroethylene emulsion is 40%.
Preferably, the hole injection layer material is one or a combination of two or more of tetrafluorotetracyanoquinodimethane, 7,8, 8-tetracyanoterephthalquinodimethane, and 4,4',4 ″ -tris (2-naphthylphenylamino) triphenylamine.
Preferably, the hole transport layer material is one or a combination of two or more of N, N '-diphenyl-N, N' - (1-naphthyl) -1,1 '-biphenyl-4, 4' -diamine, N '-diphenyl-N, N' -bis (3-methylphenyl) -1,1 '-biphenyl-4, 4' -diamine, 4 '-cyclohexylbis [ N, N-bis (4-methylphenyl) aniline ], N' -diphenyl-N, N '-bis (4-methylphenyl) biphenyl-4, 4' -diamine.
Preferably, the hole transport layer material ink is dispersed with silica aerogel, wherein the mass fraction of the silica aerogel in the ink is 0.5-1%;
preferably, the red, green and blue luminescent material inks are inks formulated by conventional OLED luminescent organic small molecules and organic polymers.
Preferably, the electron injection layer material is yttrium fluoride.
Preferably, the electron transport layer material is one or a combination of more than two of 2, 9-dimethyl-4, 7-biphenyl-1, 10-phenanthroline, 4, 7-diphenyl-1, 10-phenanthroline, 1,3, 5-tris (1-phenyl-1H-benzimidazol-2-yl) benzene, 8-hydroxyquinoline aluminum, bis (2-methyl-8-hydroxyquinoline-N1, O8) - (1,1' -biphenyl-4-hydroxy) aluminum.
The ink is prepared by a known technique and is not particularly limited. The invention uniformly selects polytetrafluoroethylene emulsion as a base solution to disperse and prepare various inks.
Preferably, the film deposited with the alloy is a polytetrafluoroethylene film deposited with one of lithium, magnesium, calcium, strontium, aluminum and indium, or a composite film of polytetrafluoroethylene and an alloy of copper, gold and silver, and a metal layer of the composite film is tightly attached to the electron transport layer through hot pressing.
Preferably, the pre-baking is performed by baking so that the coating liquid does not flow.
In the known traditional printing method, the hole transport material ink and the hole injection layer material ink are laminated by layer coating, so that the transport efficiency is low. Ink jet printing refers to the process of ejecting ink from a nozzle by an ink pump under pressure to form a continuous stream of ink that is electrostatically charged in a high voltage metal tube in a printhead to form an ordered stream of ink droplets. The pressure of the ink pump and the magnitude of the voltage are adjusted to produce as many microdroplets as possible, which are charged as the drop stream passes through the high voltage conduit, while the large drops are not. Once the charging signal is removed, the charged micro ink drops are deflected under the action of the DC electric field of the deflection electrode to form a printing ink beam which is jetted onto a printing stock to finish printing. The invention prints the figure through controlling the ink, print the material ink of hole transport material, hole injection layer material ink in the identity layer, distribute alternately, help to promote the transport efficiency of the hole.
In the same way, the invention prints the ink of the electron injection layer and the ink of the electron transmission material on one surface layer, and the surface layers are distributed at intervals, thereby being beneficial to improving the electron transmission efficiency.
Furthermore, when direct ink-jet printing is adopted, due to the change of the material of the electronic ink and the change of the printing base material, the defects of uneven printing, easy coffee effect formation and untight combination often exist. The invention creatively disperses the silicon dioxide aerogel in the ink of the hole transport layer material, and the silicon dioxide aerogel is microporous, so that the printed luminous layer can be adsorbed in time, the uneven thickness of the ink of the luminous layer during flowing is prevented, and the coffee effect is prevented from being formed.
The invention provides a method for continuously printing an OLED flexible display panel in a roll-to-roll mode, which has the outstanding characteristics and excellent effects compared with the prior art:
1. according to the preparation method, in the ink-jet printing, the microporous silicon dioxide aerogel is dispersed in the transmission material ink, so that the printed luminescent material is timely and fixedly adsorbed, the coffee effect with uneven thickness in the ink micro-leveling is prevented, and the defects of uneven printing, easy formation of coffee effect and untight combination in the direct ink-jet printing are overcome.
2. According to the preparation method, the ink of the hole injection layer material and the ink of the hole transport material are printed on one surface layer alternately through ink-jet printing, and the ink of the electron injection layer and the ink of the electron transport material are also printed on one surface layer alternately, so that the transmission efficiency is improved.
3. The preparation method disclosed by the invention combines blade coating and ink-jet printing in the roll-to-roll printing process, greatly realizes the controllability of thickness and precision, and is suitable for preparing large-area OLED flexible display devices.
Drawings
FIG. 1: the invention is a print coat of a hole transport layer, wherein: 1-hole transport material ink; 2-hole injection layer material ink;
FIG. 2: example 1 a print surface photo of a printed matter after ink-jet printing of a luminescent material layer;
FIG. 3: comparative example 1 a print surface real photograph after ink-jet printing of a luminescent material layer.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but it should not be construed that the scope of the present invention is limited to the following examples. Various substitutions and alterations can be made by those skilled in the art and by conventional means without departing from the spirit of the method of the invention described above.
Example 1
(1) Feeding the coiled polyimide film into a roll-to-roll continuous printing device, firstly, carrying out blade coating to ensure that polytetrafluoroethylene emulsion with 40 percent of solid content dispersed with graphene is coated on the surface of the polyimide film by a scraping way, and then carrying out pre-drying treatment to ensure that the coating liquid does not flow; the mass fraction of the graphene in the emulsion is 4%;
(2) through non-contact ink-jet printing, as shown in fig. 1, a hole injection material ink 2 tetrafluorotetracyanoquinodimethane ink and a hole transport material ink 1N, N '-diphenyl-N, N' - (1-naphthyl) -1,1 '-biphenyl-4, 4' -diamine ink containing silica aerogel are alternately printed on the surface of an anode at one time, and are dried to form a hole transport layer; wherein the mass fraction of the silicon dioxide aerogel in the ink is 0.5 percent;
(3) printing red, green and blue luminescent material inks on the surface of the hole transport layer according to high pixel settings through non-contact ink-jet printing, and drying;
(4) alternately printing yttrium fluoride ink and 2, 9-dimethyl-4, 7-biphenyl-1, 10-phenanthroline ink on the surface of the anode at one time, and drying to form an electron transmission layer;
(5) and pressing the polytetrafluoroethylene film deposited with the lithium and the copper on the electron transmission layer to form a cathode, and performing roller heat setting, packaging and coiling to obtain the OLED flexible display panel.
As can be seen from fig. 1, the hole transport material ink and the hole injection layer material ink of the present invention are different from the conventional layer-by-layer coating and laminating, but the hole transport material ink and the hole injection layer material ink are printed on the same layer by using a printing process and controlling the ink printing pattern, and are distributed alternately, which is beneficial to improving the transmission efficiency.
Example 2
(1) Feeding the coiled polyimide film into a roll-to-roll continuous printing device, firstly, carrying out blade coating to ensure that polytetrafluoroethylene emulsion with 40 percent of solid content dispersed with graphene is coated on the surface of the polyimide film by a scraping way, and then carrying out pre-drying treatment to ensure that the coating liquid does not flow; the mass fraction of the graphene in the emulsion is 2%;
(2) printing 7,7, 7,8, 8-tetracyano-p-phenylenediamine dimethane ink and N, N '-diphenyl-N, N' -di (3-methylphenyl) -1,1 '-biphenyl-4, 4' -diamine ink containing silicon dioxide aerogel on the surface of the anode at intervals at one time by non-contact ink-jet printing, and drying to form a hole transport layer; wherein the mass fraction of the silicon dioxide aerogel in the ink is 0.5 percent;
(3) printing red, green and blue luminescent material inks on the surface of the hole transport layer according to high pixel settings through non-contact ink-jet printing, and drying;
(4) alternately printing yttrium fluoride ink and 4, 7-diphenyl-1, 10-phenanthroline ink on the surface of the anode at one time, and drying to form an electron transmission layer;
(5) and pressing the polytetrafluoroethylene film deposited with the magnesium and the silver on the electron transmission layer to form a cathode, and performing roller heat setting, packaging and coiling to obtain the OLED flexible display panel.
Example 3
(1) Feeding the coiled polyimide film into a roll-to-roll continuous printing device, firstly, carrying out blade coating to ensure that polytetrafluoroethylene emulsion with 40 percent of solid content dispersed with graphene is coated on the surface of the polyimide film by a scraping way, and then carrying out pre-drying treatment to ensure that the coating liquid does not flow; the mass fraction of the graphene in the emulsion is 3%;
(2) printing 4,4',4' '-tri (2-naphthyl phenylamino) triphenylamine ink and 4,4' -cyclohexyl di [ N, N-di (4-methylphenyl) aniline ] ink containing silica aerogel on the surface of the anode at intervals by non-contact ink-jet printing, and drying to form a hole transport layer; wherein the mass fraction of the silicon dioxide aerogel in the ink is 0.5 percent;
(3) printing red, green and blue luminescent material inks on the surface of the hole transport layer according to high pixel settings through non-contact ink-jet printing, and drying;
(4) the zinc oxide ink and the 1,3, 5-tri (1-phenyl-1H-benzimidazole-2-yl) benzene ink are alternately printed on the surface of the anode at one time and dried to form an electron transmission layer;
(5) and pressing the polytetrafluoroethylene film deposited with the calcium and the gold on the electron transmission layer to form a cathode, and performing roller heat setting, packaging and coiling to obtain the OLED flexible display panel.
Example 4
(1) Feeding the coiled polyimide film into a roll-to-roll continuous printing device, firstly, carrying out blade coating to ensure that polytetrafluoroethylene emulsion with 40 percent of solid content dispersed with graphene is coated on the surface of the polyimide film by a scraping way, and then carrying out pre-drying treatment to ensure that the coating liquid does not flow; the mass fraction of the graphene in the emulsion is 2%;
(2) through non-contact ink-jet printing, tetrafluoro tetracyanoquinone dimethane ink and N, N ' -diphenyl-N, N ' -bis (4-methylphenyl) biphenyl-4, 4' -diamine ink containing silicon dioxide aerogel are alternately printed on the surface of an anode at one time, and are dried to form a hole transport layer; wherein the mass fraction of the silicon dioxide aerogel in the ink is 0.5 percent;
(3) printing red, green and blue luminescent material inks on the surface of the hole transport layer according to high pixel settings through non-contact ink-jet printing, and drying;
(4) the zinc oxide ink and the bis (2-methyl-8-hydroxyquinoline-N1, O8) - (1,1' -biphenyl-4-hydroxy) aluminum ink are printed on the surface of the anode at one time in an alternating mode and dried to form an electron transmission layer;
(5) and pressing the polytetrafluoroethylene film deposited with the lithium and the silver on the electron transmission layer to form a cathode, and performing roller heat setting, packaging and coiling to obtain the OLED flexible display panel.
Example 5
(1) Feeding the coiled polyimide film into a roll-to-roll continuous printing device, firstly, carrying out blade coating to ensure that polytetrafluoroethylene emulsion with 40 percent of solid content dispersed with graphene is coated on the surface of the polyimide film by a scraping way, and then carrying out pre-drying treatment to ensure that the coating liquid does not flow; the mass fraction of the graphene in the emulsion is 2%;
(2) through non-contact ink-jet printing, the tetrafluoro tetracyanoquinone dimethane ink and the 4,4' -cyclohexyl bis [ N, N-bis (4-methylphenyl) aniline ] ink containing silicon dioxide aerogel are alternately printed on the surface of the anode at one time, and the anode is dried to ensure that the water content is not higher than 1 percent to form a hole transport layer; wherein the mass fraction of the silicon dioxide aerogel in the ink is 0.5 percent;
(3) printing red, green and blue luminescent material inks on the surface of the hole transport layer according to high pixel settings through non-contact ink-jet printing, and drying to ensure that the water content is not higher than 1%;
(4) the zinc oxide ink and the bis (2-methyl-8-hydroxyquinoline-N1, O8) - (1,1' -biphenyl-4-hydroxy) aluminum ink are printed on the surface of the anode at one time in an alternating mode, and the water content is dried to be not higher than 1%, so that an electron transmission layer is formed;
(5) and pressing the polytetrafluoroethylene film deposited with strontium and copper on the electron transmission layer to form a cathode, and performing roller heat setting, packaging and coiling to obtain the OLED flexible display panel.
Comparative example 1
Comparative example 1 in comparison with example 1, no silica aerogel powder was added to the hole transport material ink, and the rest was completely the same as example 1.
FIG. 2 is a photograph of a printed matter of example 1 after ink-jet printing of a luminescent material layer, which has a smooth and uniform surface.
Fig. 3 shows that in comparative example 1, silica aerogel powder is not added to the hole transport material ink, and when the luminescent material layer is subjected to inkjet printing, due to lack of stable in-situ adsorption of the silica aerogel, the luminescent layer is microfluidized to form a printing surface with uneven thickness.
Claims (8)
1. A method for continuously printing OLED flexible display panels in a roll-to-roll mode is characterized in that the specific process of the printing method is as follows:
(1) feeding the coiled polyimide film into a roll-to-roll continuous printing device, firstly carrying out blade coating to enable the anode coating liquid to be blade-coated on the surface of the polyimide film, and then carrying out pre-drying treatment;
(2) through non-contact ink-jet printing, alternately printing the ink of the hole injection layer material and the ink of the hole transport layer material on the surface of the anode at one time, and drying to form a hole transport layer; the hole transport layer material ink is dispersed with silicon dioxide aerogel, wherein the mass fraction of the silicon dioxide aerogel in the ink is 0.5-1%;
(3) printing red, green and blue luminescent material inks on the surface of the hole transport layer according to high pixel settings through non-contact ink-jet printing, and drying;
(4) alternately printing the ink of the electron injection layer and the ink of the electron transmission material on the surface of the anode at one time, and drying to form an electron transmission layer;
(5) pressing the film deposited with the alloy on the electron transmission layer to form a cathode, and performing roller heat setting, packaging and coiling to obtain the OLED flexible display panel; the film deposited with the alloy is a polytetrafluoroethylene film deposited with one of lithium, magnesium, calcium, strontium, aluminum and indium, or a composite film of polytetrafluoroethylene and an alloy of copper, gold and silver, and a metal layer of the composite film is tightly attached to the electron transmission layer through hot pressing.
2. The method for roll-to-roll continuous printing of the OLED flexible display panel according to claim 1, wherein the anode coating liquid is prepared by ultrasonically dispersing graphene in polytetrafluoroethylene emulsion, wherein the mass fraction of graphene in the emulsion is 2-4%, and the solid content of the polytetrafluoroethylene emulsion is 40%.
3. The method of claim 1, wherein the hole injection layer material is one or a combination of more than two of tetrafluorotetracyanoquinodimethane, 7,8, 8-tetracyanoterephthalquinodimethane, and 4,4',4' ' -tris (2-naphthylphenylamino) triphenylamine.
4. The method of claim 1, wherein the hole transport layer material is one or a combination of two or more of N, N '-diphenyl-N, N' - (1-naphthyl) -1,1 '-biphenyl-4, 4' -diamine, N '-diphenyl-N, N' -bis (3-methylphenyl) -1,1 '-biphenyl-4, 4' -diamine, 4 '-cyclohexylbis [ N, N-bis (4-methylphenyl) aniline ], N' -diphenyl-N, N '-bis (4-methylphenyl) biphenyl-4, 4' -diamine.
5. The method of claim 1, wherein the red, green and blue emissive material inks are conventional OLED emissive small organic molecule, organic polymer formulated inks.
6. The method of claim 1, wherein the electron injection layer material is yttrium fluoride.
7. The method of claim 1, wherein the electron transport layer material is one or a combination of two or more of 2, 9-dimethyl-4, 7-biphenyl-1, 10-phenanthroline, 4, 7-diphenyl-1, 10-phenanthroline, 1,3, 5-tris (1-phenyl-1H-benzimidazol-2-yl) benzene, 8-hydroxyquinoline aluminum, bis (2-methyl-8-hydroxyquinoline-N1, O8) - (1,1' -biphenyl-4-hydroxy) aluminum.
8. The method for roll-to-roll continuous printing of the OLED flexible display panel according to claim 1, wherein the pre-drying means drying to make the coating liquid not flow.
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| US20100314994A1 (en) * | 2009-06-16 | 2010-12-16 | Chi Ming Che | Platinum (II) Isoqulinoline-Pyridine-Benzene Based Complexes, Methods for Making Same, and Organic Light-Emitting Diodes Including Such Complexes |
| CN107275499A (en) * | 2017-06-12 | 2017-10-20 | 广州琉芯光电科技有限公司 | A kind of light emitting diode with quantum dots and preparation method thereof |
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| US20100314994A1 (en) * | 2009-06-16 | 2010-12-16 | Chi Ming Che | Platinum (II) Isoqulinoline-Pyridine-Benzene Based Complexes, Methods for Making Same, and Organic Light-Emitting Diodes Including Such Complexes |
| CN107275499A (en) * | 2017-06-12 | 2017-10-20 | 广州琉芯光电科技有限公司 | A kind of light emitting diode with quantum dots and preparation method thereof |
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